CN101962478A - Polyimide film and production process thereof - Google Patents
Polyimide film and production process thereof Download PDFInfo
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- CN101962478A CN101962478A CN 201010284219 CN201010284219A CN101962478A CN 101962478 A CN101962478 A CN 101962478A CN 201010284219 CN201010284219 CN 201010284219 CN 201010284219 A CN201010284219 A CN 201010284219A CN 101962478 A CN101962478 A CN 101962478A
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- Prior art keywords
- tetracarboxylic dianhydride
- bibenzene tetracarboxylic
- film
- solvent
- kapton
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 229920001721 polyimide Polymers 0.000 title abstract 3
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000011347 resin Substances 0.000 claims abstract description 38
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000005303 weighing Methods 0.000 claims abstract description 17
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 12
- 125000005462 imide group Chemical group 0.000 claims abstract description 11
- 230000001105 regulatory effect Effects 0.000 claims abstract description 8
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 42
- 125000006158 tetracarboxylic acid group Chemical group 0.000 claims description 42
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 29
- YVNRUPSDZZZUQJ-UHFFFAOYSA-N [O].NC1=CC=CC=C1 Chemical compound [O].NC1=CC=CC=C1 YVNRUPSDZZZUQJ-UHFFFAOYSA-N 0.000 claims description 20
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 206010039424 Salivary hypersecretion Diseases 0.000 claims description 2
- 208000026451 salivation Diseases 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000005266 casting Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 12
- LDFYRFKAYFZVNH-UHFFFAOYSA-N 4-[4-[4-(4-aminophenoxy)phenoxy]phenoxy]aniline Chemical compound C1=CC(N)=CC=C1OC(C=C1)=CC=C1OC(C=C1)=CC=C1OC1=CC=C(N)C=C1 LDFYRFKAYFZVNH-UHFFFAOYSA-N 0.000 abstract 1
- JVERADGGGBYHNP-UHFFFAOYSA-N 5-phenylbenzene-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(=O)O)=CC(C=2C=CC=CC=2)=C1C(O)=O JVERADGGGBYHNP-UHFFFAOYSA-N 0.000 abstract 1
- 229940113088 dimethylacetamide Drugs 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- 238000005070 sampling Methods 0.000 description 9
- 239000002994 raw material Substances 0.000 description 5
- 150000003949 imides Chemical class 0.000 description 4
- 230000008901 benefit Effects 0.000 description 2
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention relates to a polyimide film and a production process thereof. The polyimide film is mainly formed by the polymerization of material A 4,4'-bis(4-aminophenoxy)diphenylether and material B biphenyl tetracarboxylic acid dianhydride, wherein the ratio of the number of imide groups to the molecular weight of chain links is 2/678. The production process comprises the following steps: weighing the material A and the material b according to a weight ratio of 1.3:(0.99-1.0), and using N,N'-dimethyl acetamide as a solvent; throwing the material A into the solvent, stirring until the material A is dissolved, throwing the material B into the solvent in multiple times at a time interval of 20-50 minutes, and stirring, wherein the temperature is limited to 20-70 DEG C, and the weight of the solvent is 3-9 times of the total weight of the material A and the material B; and stopping throwing the material B when the resin viscosity reaches the reaction end point (4.0-7.0*10<5> centipoises) at 30 DEG C, continuing to stir for 4-6 hours to obtain a polyamic acid resin solution, casting into a film, and carrying out imidization; and regulating the viscosity when the material B remains 0.3-0.5 kilogram, wherein 0.03-0.1 kilogram of the material B is thrown each time, and the throwing amount is gradually reduced. The imide group content of the film is greatly reduced, and the alkali resistance and the moisture resistance of the film are greatly improved.
Description
(1) technical field
The present invention relates to the plastics film manufacturing technology, be specially a kind of Kapton and production technique thereof.
(2) background technology
Kapton is a kind of insulating material of excellent heat resistance, and it is widely used in industries such as electronics, electrician, space flight and aviation; Traditional product mainly is equal benzene type Kapton, and its share of market reaches more than 80%, pyromellitic acid anhydride and 4 in its raw material, and the weight ratio of 4 '-diaminodiphenyl oxide is 218 to 200, the imide group number is 2/418 with the ratio of chain link molecular weight.With N, N '-N,N-DIMETHYLACETAMIDE is solvent, carry out polycondensation, and synthetic polyamic acid resin solution with gained resin solution hydrostomia film forming and through operations such as imidizations, obtains equal benzene type Kapton product then.The imide mass contg height of this series products, so alkali resistance and moisture resistivity are relatively poor has influenced its application at some special dimensions.
(3) summary of the invention
The purpose of this invention is to provide a kind of Kapton, mainly by 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride are polymerized, and compare equal its imide mass contg of benzene type Kapton and obviously reduce, and therefore alkaline-resisting and anti-moisture performance has improved.
Another object of the present invention provides a kind of Kapton production technique, and main raw material is 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride.
Kapton of the present invention mainly is polymerized by 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride, and wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
Kapton production technique of the present invention comprises the steps:
I, weighing
Be 1.3 by weight: (0.99～1.0) takes by weighing 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride; Solvent is N, N '-N,N-DIMETHYLACETAMIDE.
II, preparation resin solution
Earlier 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped into solvent N, in N '-N,N-DIMETHYLACETAMIDE, stir and make its thorough dissolving, drop into bibenzene tetracarboxylic dianhydride then several times and stir each 20～50 minutes at interval; Control reaction temperature is 20 ℃～70 ℃ in the process that feeds intake.Resin viscosity reaches 4.0～7.0 ten thousand centipoises and then is reaction end when 30 ℃ of temperature, stop to drop into bibenzene tetracarboxylic dianhydride, continues to stir 4～6 hours, promptly obtains polyamic acid resin solution, enters film making process behind the froth breaking.
III, film forming
The polyamic acid resin solution of Step II gained is technology hydrostomia film forming routinely;
IV, imidization
The salivation film of Step II I gained technology routinely carries out imidization.
Described step I takes by weighing solvent N, and the weight of N '-N,N-DIMETHYLACETAMIDE is 3～9 times of above-mentioned two kinds of raw material gross weights.
Bibenzene tetracarboxylic dianhydride drops into several times in the described Step II; First input amount be among the step I amount of getting 40%～55%, drop into once at every afterwards interval 20～50 minutes, each input amount is 40%～55% of a remaining bibenzene tetracarboxylic dianhydride amount.
When 0.3～0.5 kilogram of bibenzene tetracarboxylic dianhydride residue, regulate viscosity in the described Step II, only drop into 0.03～0.1 kilogram at every turn, stir and detect resin viscosity after 20～40 minutes, reaching 4.0～7.0 ten thousand centipoises when 30 ℃ of temperature is reaction end.The input amount of bibenzene tetracarboxylic dianhydride reduces gradually when regulating viscosity, in order to avoid the resin viscosity sudden change makes the excessive input of raw material.
The advantage of Kapton of the present invention is: the imide mass contg only is 62% of the equal benzene type Kapton of tradition in this Kapton, significantly minimizing because of the imide mass contg, make this Kapton alkali resistance and moisture resistivity all be greatly improved, satisfy the application requiring under the special environment condition.
The advantage of Kapton production technique of the present invention is: 1, raw materials used with traditional equal benzene type Kapton is different, by 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride are after polycondensation, again through casting film-forming and imidization and make film; The content of this technology gained film imide group reduces, and performance improves, and satisfies the application requiring under the special environment condition; 2, be applicable to that making thickness is 0.005mm～0.35mm, fabric width is the Kapton product of 500mm～1500mm.
(4) embodiment
Embodiment 1:
I, weighing
Take by weighing 4,4 of 14.3kg '-two (4-amino-benzene oxygen) phenyl ether and 11kg bibenzene tetracarboxylic dianhydride; Solvent N, N '-N,N-DIMETHYLACETAMIDE 75kg;
II, preparation resin solution
Use has cooling water circulation reactor, and the N that 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped in N '-N,N-DIMETHYLACETAMIDE, stirs and makes its thorough dissolving earlier; Drop into bibenzene tetracarboxylic dianhydride and stirring then, control reaction temperature is between 20 ℃ to 70 ℃ in batches; Dropping into bibenzene tetracarboxylic dianhydride first is 5.5kg, dropped into for the second time in 50 minutes at interval, input amount is 2.8kg, dropped into for the third time in 50 minutes at interval again, input amount is 1.4kg, drop into for 50 minutes the 4th time at interval again, input amount is 0.7kg, drops into for 50 minutes the 5th time at interval again, and input amount is 0.3kg, last 0.4kg BPDA is used for regulating viscosity, promptly begin a small amount of input, drop into for 40 minutes the 6th time at interval, input amount is 0.1kg, stir 40 minutes sampling and measuring resin viscosities and do not reach 40,000 centipoises yet, then drop into for the 7th time, input amount is 0.05kg, stirs 40 minutes sampling and measuring resin viscosities, viscosity reached 4.0 ten thousand centipoises when resin was spent in temperature 30, this is a reaction end, and remaining bibenzene tetracarboxylic dianhydride no longer drops into, and continues to stir 6 hours, promptly obtain polyamic acid resin solution, will promptly can carry out next step film making process behind its froth breaking.
III, film forming
By traditional technology with the hydrostomia mouth with polyamic acid resin solution on the ring-like Stainless Steel Band of slobbering machine equably stream become one deck liquid film, send into again and with hot blast solvent dried in the drying tunnel; Remaining solvent is controlled at 25%, after the week of circulating film is stripped down from steel band;
IV, imidization
Send into the imidization stove by traditional technology from the film that the ring-like Stainless Steel Band of slobbering machine strips down, finish imidization film take-up, detect, finished product warehouse-in.
The gained Kapton after testing, wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
Embodiment 2:
I, weighing
Take by weighing 4,4 of 11.3kg '-two (4-amino-benzene oxygen) phenyl ether and 8.7kg bibenzene tetracarboxylic dianhydride; Solvent N, N '-N,N-DIMETHYLACETAMIDE 80kg;
II, preparation resin solution
Use has cooling water circulation reactor, earlier 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped into N, in N '-N,N-DIMETHYLACETAMIDE, stirs and makes its thorough dissolving; Drop into bibenzene tetracarboxylic dianhydride and stirring then, control reaction temperature is between 20 ℃ to 70 ℃ in batches; Dropping into bibenzene tetracarboxylic dianhydride first is 4.4kg, dropped into for the second time in 40 minutes at interval, input amount is 2.3kg, dropped into for the third time in 30 minutes at interval, input amount is 1.1kg again, drops into for 30 minutes the 4th time at interval again, input amount is 0.6kg, remaining 0.3kg bibenzene tetracarboxylic dianhydride is used for regulating viscosity, drops into for 30 minutes the 5th time at interval, and input amount is 0.1kg, stir sampling and measuring resin viscosity after 30 minutes, do not reach requirement, then drop into for the 6th time, input amount is 0.08kg, stirred 30 minutes, measuring resin is 30 ℃ in temperature, and viscosity reaches 5.0 ten thousand centipoises, and this is a reaction end, remaining bibenzene tetracarboxylic dianhydride no longer drops into, continue to stir 5 hours, promptly obtain polyamic acid resin solution, will promptly can carry out next step film making process behind its froth breaking.
III, film forming
Press the technology hydrostomia film forming of embodiment 1;
IV, imidization
Technology by embodiment 1 is carried out imidization, afterwards film take-up, detect, finished product warehouse-in.
The gained Kapton after testing, wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
Embodiment 3:
I, weighing
Take by weighing 4,4 of 5.65kg '-two (4-amino-benzene oxygen) phenyl ether and 4.35kg bibenzene tetracarboxylic dianhydride; Solvent N, N '-N,N-DIMETHYLACETAMIDE 90kg;
II, preparation resin solution
Use has cooling water circulation reactor, and the N that 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped in N '-N,N-DIMETHYLACETAMIDE, stirs and makes its thorough dissolving earlier; Drop into bibenzene tetracarboxylic dianhydride and stirring then, control reaction temperature is between 20 ℃ to 70 ℃ in batches; Dropping into bibenzene tetracarboxylic dianhydride first is 2.2kg, drops into for the second time in 30 minutes at interval, and input amount is 1.1kg, dropped into for the third time in 40 minutes at interval, input amount is 0.55kg again, and remaining 0.5kg bibenzene tetracarboxylic dianhydride is used for regulating viscosity, drop into for 20 minutes the 4th time at interval, input amount is 0.1kg, stirs sampling and measuring resin viscosity after 20 minutes, do not reach requirement, drop into for the 5th time, input amount is 0.1kg, stirs 20 minutes, the sampling and measuring resin viscosity does not reach requirement yet; Drop into for the 6th time again, input amount is 0.03kg, stir after 20 minutes and to be 30 ℃ in temperature and to measure resin viscosities, viscosity reaches 7.0 ten thousand centipoises, this is a reaction end, and remaining bibenzene tetracarboxylic dianhydride no longer drops into, and continues to stir 4 hours, promptly obtain polyamic acid resin solution, will promptly can carry out next step film making process behind its froth breaking.
III, film forming
Press the technology hydrostomia film forming of embodiment 1;
IV, imidization
Technology by embodiment 1 is carried out imidization, afterwards film take-up, detect, finished product warehouse-in.
The gained Kapton after testing, wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
Embodiment 4:
I, weighing
Take by weighing 4,4 of 5.65kg '-two (4-amino-benzene oxygen) phenyl ether and 4.30kg bibenzene tetracarboxylic dianhydride; Solvent N, N '-N,N-DIMETHYLACETAMIDE 50kg;
II, preparation resin solution
Use has cooling water circulation reactor, and the N that 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped in N '-N,N-DIMETHYLACETAMIDE, stirs and makes its thorough dissolving earlier; Drop into bibenzene tetracarboxylic dianhydride and stirring then, control reaction temperature is between 20 ℃ to 70 ℃ in batches; Dropping into bibenzene tetracarboxylic dianhydride first is 2.2kg, dropped into for the second time in 30 minutes at interval, input amount is 1.2kg, dropped into for the third time in 40 minutes at interval again, input amount is 0.5kg, remaining 0.4kg bibenzene tetracarboxylic dianhydride is used for regulating viscosity, dropped on a small quantity in 30 minutes at interval at every turn, stir back sampling and measuring resin viscosity, input amount is 0.1kg successively, 0.1kg, 0.1kg, 0.05kg, 0.03kg, 0.02kg, stir back sampling and measuring resin viscosity at last, be under 30 ℃ in temperature, viscosity reaches 6.1 ten thousand centipoises, this is a reaction end, and bibenzene tetracarboxylic dianhydride does not have residue, continues to stir 4 hours, promptly obtain polyamic acid resin solution, will promptly can carry out next step film making process behind its froth breaking.
III, film forming
Press the technology hydrostomia film forming of embodiment 1;
IV, imidization
Technology by embodiment 1 is carried out imidization, afterwards film take-up, detect, finished product warehouse-in.
The gained Kapton after testing, wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
Embodiment 5:
I, weighing
Take by weighing 4,4 of 14.3kg '-two (4-amino-benzene oxygen) phenyl ether and 10.95kg bibenzene tetracarboxylic dianhydride; Solvent N, N '-N,N-DIMETHYLACETAMIDE 75kg;
II, preparation resin solution
Use has cooling water circulation reactor, and the N that 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped in N '-N,N-DIMETHYLACETAMIDE, stirs and makes its thorough dissolving earlier; Drop into bibenzene tetracarboxylic dianhydride and stirring then, control reaction temperature is between 20 ℃ to 70 ℃ in batches; Dropping into bibenzene tetracarboxylic dianhydride first is 5.5kg, dropped into for the second time in 50 minutes at interval, input amount is 2.8kg, dropped into for the third time in 50 minutes at interval, input amount is 1.4kg again, drops into for 50 minutes the 4th time at interval again, input amount is 0.7kg, drop into for 50 minutes the 5th time at interval, input amount is 0.3kg again, and last 0.35kg BPDA is used for regulating viscosity, dropped on a small quantity in 40 minutes at interval at every turn, stir back sampling and measuring resin viscosity, input amount is 0.1kg successively, 0.05kg, 0.05kg, 0.03kg, 0.01kg, stir back sampling and measuring resin viscosity at last, in temperature is under 30 ℃, viscosity reaches 6.4 ten thousand centipoises, and this is a reaction end, and this is a reaction end, remaining bibenzene tetracarboxylic dianhydride no longer drops into, continue to stir 6 hours, promptly obtain polyamic acid resin solution, will promptly can carry out next step film making process behind its froth breaking.
III, film forming
Press the technology hydrostomia film forming of embodiment 1;
IV, imidization
Technology by embodiment 1 is carried out imidization, afterwards film take-up, detect, finished product warehouse-in.
The gained Kapton after testing, wherein the imide group number is 2/678 with the ratio of chain link molecular weight.
The foregoing description is the specific case that purpose of the present invention, technical scheme and beneficial effect are further described only, and the present invention is defined in this.All any modifications of within scope of disclosure of the present invention, being made, be equal to replacement, improvement etc., all be included within protection scope of the present invention.
Claims (7)
1. Kapton is characterized in that:
Mainly be polymerized by 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride, its imide group number is 2/678 with the ratio of chain link molecular weight.
2. the Kapton production technique is characterized in that comprising the steps:
I, batching
Be 1.3 by weight: (0.99～1.0) takes by weighing 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride; Solvent is N, N '-N,N-DIMETHYLACETAMIDE;
II, preparation resin solution
Earlier 4,4 '-two (4-amino-benzene oxygen) phenyl ether is dropped into solvent N, in N '-N,N-DIMETHYLACETAMIDE, stirring makes its thorough dissolving, drop into bibenzene tetracarboxylic dianhydride and stirring then several times, each 20～50 minutes at interval, control reaction temperature was 20 ℃～70 ℃ in the process that feeds intake; Resin viscosity is a reaction end when reaching 4.0～7.0 ten thousand centipoises for 30 ℃, stops to drop into bibenzene tetracarboxylic dianhydride, continues to stir 4～6 hours, promptly obtains polyamic acid resin solution, enters film making process behind the froth breaking;
III, film forming
The polyamic acid resin solution hydrostomia film forming of Step II gained;
IV, imidization
The salivation film of Step II I gained carries out imidization, afterwards film take-up, finished product.
3. Kapton production technique according to claim 2 is characterized in that:
Take by weighing solvent N among the described step I, the weight of N '-N,N-DIMETHYLACETAMIDE is 3～9 times that 4,4 '-two (4-amino-benzene oxygen) phenyl ether and bibenzene tetracarboxylic dianhydride take by weighing total amount.
4. according to claim 2 or 3 described Kapton production technique, it is characterized in that:
In the described Step II bibenzene tetracarboxylic dianhydride first input amount be among the step I amount of getting 40%～55%, each afterwards input amount is 40%～55% of a remaining bibenzene tetracarboxylic dianhydride amount.
5. according to claim 2 or 3 described Kapton production technique, it is characterized in that:
Regulate viscosity when bibenzene tetracarboxylic dianhydride remains 0.3～0.5 kilogram in the described Step II, only drop into 0.03～0.1 kilogram at every turn, stir the back and detect resin viscosity.
6. Kapton production technique according to claim 5 is characterized in that:
The input amount of bibenzene tetracarboxylic dianhydride reduces one by one when regulating viscosity.
7. according to claim 2 or 3 described Kapton production technique, it is characterized in that:
Described Step II is used cooling water circulation reactor.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516582A (en) * | 2011-12-21 | 2012-06-27 | 桂林电器科学研究院 | Manufacturing method of porous polyimide film |
| CN102582138A (en) * | 2012-01-18 | 2012-07-18 | 桂林电器科学研究院 | Multi-layer porous polyimide film and preparation method of porous polyimide film |
| CN103698177A (en) * | 2013-12-13 | 2014-04-02 | 河北省首钢迁安钢铁有限责任公司 | Sample processing method for measuring pulling stress on steel plate supplied by oriented silicon steel coating |
| CN108384002A (en) * | 2017-02-03 | 2018-08-10 | 台虹科技股份有限公司 | Polyimide polymer and polyimide film |
| CN111057256A (en) * | 2019-11-22 | 2020-04-24 | 桂林电器科学研究院有限公司 | Preparation method of size-stable polyimide film |
| CN114481355A (en) * | 2022-02-17 | 2022-05-13 | 苏州鸿凌达电子科技股份有限公司 | Method for preparing heat-conducting insulating film based on hexagonal boron nitride |
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| CN101402730A (en) * | 2008-11-12 | 2009-04-08 | 桂林电器科学研究所 | Synthesis of polyamic acid resin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516582A (en) * | 2011-12-21 | 2012-06-27 | 桂林电器科学研究院 | Manufacturing method of porous polyimide film |
| CN102582138A (en) * | 2012-01-18 | 2012-07-18 | 桂林电器科学研究院 | Multi-layer porous polyimide film and preparation method of porous polyimide film |
| CN102582138B (en) * | 2012-01-18 | 2015-05-27 | 桂林电器科学研究院有限公司 | Multi-layer porous polyimide film and preparation method of porous polyimide film |
| CN103698177A (en) * | 2013-12-13 | 2014-04-02 | 河北省首钢迁安钢铁有限责任公司 | Sample processing method for measuring pulling stress on steel plate supplied by oriented silicon steel coating |
| CN108384002A (en) * | 2017-02-03 | 2018-08-10 | 台虹科技股份有限公司 | Polyimide polymer and polyimide film |
| CN111057256A (en) * | 2019-11-22 | 2020-04-24 | 桂林电器科学研究院有限公司 | Preparation method of size-stable polyimide film |
| CN111057256B (en) * | 2019-11-22 | 2021-01-15 | 桂林电器科学研究院有限公司 | Preparation method of size-stable polyimide film |
| CN114481355A (en) * | 2022-02-17 | 2022-05-13 | 苏州鸿凌达电子科技股份有限公司 | Method for preparing heat-conducting insulating film based on hexagonal boron nitride |
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| CN101962478B (en) | 2012-10-03 |
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